CN108933251A - A kind of biomass carbon/ferric oxide composite material and preparation method thereof - Google Patents
A kind of biomass carbon/ferric oxide composite material and preparation method thereof Download PDFInfo
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- CN108933251A CN108933251A CN201810995604.2A CN201810995604A CN108933251A CN 108933251 A CN108933251 A CN 108933251A CN 201810995604 A CN201810995604 A CN 201810995604A CN 108933251 A CN108933251 A CN 108933251A
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a kind of cathode of lithium battery biomass carbon/ferric oxide composite material and preparation method thereof, the problem of it is big to solve lithium cell cathode material iron oxide cubical expansivity, poor circulation.Biomass carbon is made in the carbonizations such as leaf, bark, chips and/or animal hair, it is using forced hydro-thermal method that biomass carbon is compound with iron oxide again, obtain the carbon-coated iron oxide presoma of multiporous biological matter, then presoma is changed into iron oxide crystallinity by microwave treatment, obtains biomass carbon/ferric oxide composite material of the present invention.Biomass carbon/ferric oxide composite material prepared by the present invention is low in cost, may be directly applied in the electrode material of negative electrode of lithium ion battery, has extensive practical application value and industrial production prospect.
Description
Technical field
The invention belongs to battery critical material and technical fields, and in particular to a kind of ion secondary battery cathode material lithium and
Preparation method, more particularly to a kind of biomass carbon/ferric oxide composite material and preparation method thereof.
Background technique
Inexpensively, high-energy density and be that the following power battery is extensive with the electrode material of good cyclical stability
The important prerequisite of application.In order to improve battery performance and reduce production prices, need to develop high capacity, long-life, low price
Lithium cell cathode material.
Iron oxide is widely used in various aspects due to its natural resources abundant, hypotoxicity and excellent performance.Closely
Over a little years, it is widely studied since it has excellent chemical property as lithium cell cathode material.Many different-shapes
Iron oxide material be synthesized by different synthetic methods.For example, the rod-like iron oxide and hydro-thermal legal system of microwave method preparation
Standby iron oxide.Although iron oxide specific capacity is up to 1008mAh/g, it acutely begins as oxide material, volume expansion
It is inevitable problem eventually, volume expansion drastically reduces circulating battery specific capacity, so most of pure iron oxide materials
Specific capacity is always in 300mAh/g or so, although the obtained iron oxide specific capacity of solvent-thermal method can achieve the left side 600mAh/g
The right side, but high production cost and low yield makes it not have use value.Therefore more and more researchs now, which are absorbed in, changes
It is apt to its cycle performance, main path is carbon material to be added and iron oxide is compound obtains oxidation of coal iron composite material.
Nowadays carbon material type is especially more, and economy can be brought by finding cheap carbon source and developing its application value
Benefit.Biomass carbon has inborn advantage than other carbon materials as the reproducible resource of nature, price and resource, passes through
The very high carbon material of the available specific capacity of activation of activating substance such as KOH, KCl, NaOH, nowadays there are many biomass carbons
Material is studied as lithium cell cathode material.Various leaves, bark and chips, such as: the leaf of bamboo, Chinese parasol leaf, pine
Bark, oriental plane tree wood chip etc. and animal hair are all the materials being easy to get, and from a wealth of sources, the cleaning of leaf and bark
It is that annual cost manpower is needed to go cleaning and embedding treatment with embedding, the waste materials such as leaf, bark and chips is carbonized
Using waste utilization may be implemented.
Summary of the invention
Low, poor circulation that it is an object of the invention to the iron oxide conductivity for overcoming existing carbon material compound, volume are swollen
The drawbacks of swelling proposes a kind of biomass carbon/ferric oxide composite material and preparation method thereof.
It is an object of the present invention to provide a kind of biomass carbon/ferric oxide composite materials, it is characterised in that: including biology
Matter carbon substrate and the iron oxide being attached in substrate, the iron oxide is distributed in the porous structure of biomass carbon, wherein giving birth to
Substance carbon accounting 20%~50%.
Further, in the composite material biomass carbon porous structure, hole diameter be 7~10um.
Further, in the composite material iron oxide be rodlike, 50~150nm of granular size, in normal distribution in
The two sides 70nm, are evenly distributed among the hole of biomass carbon, form nanostructure.
It is a further object to provide a kind of preparation method of biomass carbon/ferric oxide composite material, features
It is, it is using forced hydro-thermal method that biomass carbon is compound with iron oxide, the carbon-coated iron oxide presoma of multiporous biological matter is obtained,
Then presoma is improved into iron oxide crystallinity by microwave treatment, it is compound obtains biomass carbon/iron oxide of the present invention
Material.
The preparation method of a kind of biomass carbon/ferric oxide composite material of the invention, by forcing hydro-thermal method and microwave method
It combines, biomass carbon is compound with iron oxide, to improve the electronics and ionic conductivity of iron oxide, and charge and discharge are limited simultaneously
When volume expansion, and then improve material circulation performance and improve material specific capacity.
It is specifically described a kind of preparation method of biomass carbon/ferric oxide composite material provided by the invention again, including with
Lower step:
(1) 0.1~1.5g biomass carbon is added to the NaH that 300~500ml concentration is 0.03~0.07 g/L2PO4Aqueous solution
In, the FeCl that 3.6~10.8ml concentration is 1~3mol/L is then added dropwise3Solution, oil bath heating stir 1~3h simultaneously.
(2) solution for taking out step (1) is allowed to be cooled to room temperature, is then placed in micro-wave oven the microwave at 800~900W
10~20min is handled, finally by being centrifuged, being filtered, washed, drying, it is compound that biomass carbon/iron oxide of the invention can be obtained
Material.
A kind of preparation method of biomass carbon/ferric oxide composite material, further includes the preparation method of biomass carbon,
The following steps are included:
(1) leaf collected, bark, chips and/or animal hair are cleaned with deionized water, with 0.5~1.5mol/L's
Potassium hydroxide solution impregnates 20~48h, is then placed in 70~90 DEG C of drying in drying box.
(2) sample of drying is collected in ceramic vessel, is placed in calcining furnace under ar gas environment and forges for 800~950 DEG C
Burn 2~4h.
(3) it is then washed with the hydrochloric acid solution of 0.5~1.5mol/L and deionized water until the aobvious neutrality of filtrate PH, is placed on dry
Dry 10~20h at 75~85 DEG C, is ground up, sieved after taking-up, biomass carbon can be obtained in dry case.
Compared with prior art, the invention has the following advantages:
Biomass carbon raw material access approaches are convenient, environmentally protective, low in cost.Preparation process is simple and convenient, and iron oxide
Compound be the required device simple by forcing hydro-thermal method combination microwave method to synthesize, easy mass production.By modified
Iron oxide has good crystallinity, and ferric oxide particles are attached on biomass carbon particle-matrix.
Biomass carbon and the compound passivation film impedance for making material of iron oxide, Charge-transfer resistance reduce, improve lithium from
Sub- diffusion rate.Biomass carbon/ferric oxide composite material prepared by the present invention is pure phase, and crystal grain distribution is uniform, is had good
Electrochemistry cycle performance.Wherein biomass carbon content be 20%-50% when, discharging condition be set as 200mA/g, 500mA/g,
Under 800mA/g, 1000mA/g, 2000mA/g, specific discharge capacity range be respectively 300~700mAh/g, 260~540mAh/
G, 220~430mAh/g, 180~360mAh/g and 120~200mAh/g.
Detailed description of the invention
Fig. 1 is the x-ray diffraction pattern according to sample made from the embodiment of the present invention 1.
Fig. 2 is the thermal multigraph according to sample made from the embodiment of the present invention 1
Fig. 3 is the scanning electron microscope diagram according to sample made from the embodiment of the present invention 1.
Fig. 4 is the transmission electron microscope figure according to sample made from the embodiment of the present invention 1
Fig. 5 is the high rate performance figure according to sample made from the present embodiment 1 and comparative example 1.In Fig. 5, abscissa is circulation time
Number, ordinate be specific discharge capacity/mAh/g, charge-discharge magnification be respectively 0.2C, 0.5C, 0.8C, 1C, 2C(200mA/g,
500mA/g, 800mA/g, 1000mA/g, 2000mA/g).
Fig. 6 is according to cycle performance figure of the sample at 0.2C made from the embodiment of the present invention 1 and comparative example 1.In Fig. 6
In, abscissa is cycle-index, and ordinate is specific discharge capacity/mAh/g.
PCB/ iron oxide is the abbreviation of Chinese parasol leaf biomass carbon/iron oxide composite in Fig. 1, Fig. 5 and Fig. 6.
Specific embodiment
The present invention is specifically described below by experiment embodiment, it is necessary to be pointed out that this example is served only for pair
The present invention is described further, and should not be understood as limiting the scope of the invention, and the person skilled in the art in the field can be with
Some nonessential modifications and adaptations are made according to the content of foregoing invention.
Embodiment 1
The Chinese parasol leaf collected is cleaned with deionized water, is then impregnated for 24 hours with the potassium hydroxide solution of 1mol/L, it is dry in air blast
80 in dry caseoC is evaporated.Then it collects and is placed in tube furnace in porcelain Noah's ark, 99% purity of argon gas, argon flow 30-
60ml/min is warming up to 900 with the heating rate of 5 DEG C/minoC calcines 2h at such a temperature.Then spend hydrochloric acid solution and from
Sub- water washing is placed on 80 in drying box until the aobvious neutrality of filtrate PHoDry 10h, is ground up, sieved to obtain phoenix tree leaf biomass under C
Carbon.It is the NaH that 400ml concentration is 0.054g/L that 0.4g phoenix tree leaf biomass carbon material, which is added to volume,2PO4In aqueous solution,
Then the FeCl that 7.2ml concentration is 1.5mol/L is added3Solution is transferred to flask oil bath agitating and heating 2h, to be cooled to arrive room temperature
After be transferred in beaker and be placed in micro-wave oven microwave treatment 10min under 900W, be finally centrifuged, be filtered, washed, be dried to obtain biology
Matter carbon/iron oxide composite.
Embodiment 2
The leaf of bamboo collected is cleaned with deionized water, then 48h is impregnated with the potassium hydroxide solution of 0.5mol/L, in forced air drying
85 in caseoC is evaporated.Then it collects and is placed in tube furnace mounted in porcelain Noah's ark, 99% purity of argon gas, argon flow 30-60ml/
Min is warming up to 950 with the heating rate of 5 DEG C/minoC calcines 2h at such a temperature.Then hydrochloric acid solution and ionized water are spent
Washing is placed on 85 in drying box until the aobvious neutrality of filtrate PHoDry 10h, is ground up, sieved, obtains leaf of bamboo biomass carbon under C.It will
0.1g biomass carbon material is added to the NaH that concentration is 0.03g/L2PO4In aqueous solution, 10.8ml concentration, which is then added, is
The FeCl of 1mol/L3Solution, is transferred to flask oil bath agitating and heating 4h, to be cooled to be placed on microwave to being transferred in beaker after room temperature
Microwave treatment 25min under 800W in furnace is finally centrifuged, is filtered, washed, being dried to obtain biomass carbon/iron oxide composite.
Embodiment 3
The hair and pine bark that the mass ratio collected is 1:1 are cleaned with deionized water, then use the potassium hydroxide of 1.5mol/L
Solution impregnates 20h, 75 in air dry ovenoC is evaporated.Then it collects and is placed in tube furnace mounted in porcelain Noah's ark, argon gas 99% is pure
Degree, argon flow 30-60ml/min are warming up to 9 800 with the heating rate of 5 DEG C/minoC calcines 4h, so at such a temperature
Afterwards.Then hydrochloric acid solution and ion water washing are spent until the aobvious neutrality of filtrate PH, is placed on 75 in drying boxoDry 20h, grinds under C
Honed sieve obtains hair and pine bark biomass carbon.1.5g hair and pine bark biomass carbon material, which are added to concentration, is
The NaH of 0.07g/L2PO4In aqueous solution, the FeCl that 3.6ml concentration is 3mol/L is then added3Solution is transferred to flask oil bath
Agitating and heating 1h, it is to be cooled to be placed in micro-wave oven microwave treatment 10min under 900W to being transferred in beaker after room temperature, finally from
The heart is filtered, washed, is dried to obtain biomass carbon/iron oxide composite
Embodiment 4
The French parasol tree and wood chip collected are cleaned with deionized water, are then impregnated with the potassium hydroxide solution of 1.5mol/L
20h, 80 in air dry ovenoC is evaporated.Then it collects and is placed in tube furnace 900 under ar gas environment in porcelain Noah's arkoC calcining
2h.Then hydrochloric acid solution and ion water washing are spent until the aobvious neutrality of filtrate PH, is placed on 80 in drying boxoDry 10h, grinds under C
Honed sieve obtains phoenix tree leaf biomass carbon.It is 400ml 0.054g/L's that 0.4g phoenix tree leaf biomass carbon, which is added to concentration,
NaH2PO4In aqueous solution, 7.2ml FeCl is then added3(1.5mol/L) is transferred to flask oil bath agitating and heating 2h, to be cooled
It is transferred to after to room temperature in beaker and is placed in micro-wave oven microwave treatment 10min under 900W, be finally centrifuged, be filtered, washed, dry
To biomass/iron oxide composite.
Comparative example 1
The Chinese parasol leaf collected is cleaned with deionized water, is then impregnated for 24 hours with the potassium hydroxide solution of 1mol/L, it is dry in air blast
80 in dry caseoC is evaporated.Then it collects and is placed in tube furnace in porcelain Noah's ark, 99% purity of argon gas, argon flow 30-
60ml/min is warming up to 900 with the heating rate of 5 DEG C/minoC calcines 2h at such a temperature.Then spend hydrochloric acid solution and from
Sub- water washing is placed on 80 in drying box until the aobvious neutrality of filtrate PHoDry 10h, is ground up, sieved to obtain phoenix tree leaf biomass under C
Carbon.By 0.0216g NaH2PO4It is dissolved in 400ml deionized water, the FeCl that 7.2ml concentration is 1.5mol/L is then added3It is molten
Liquid, while it is biomass carbon that 0.4g, which is added, is stirred evenly, is transferred to flask oil bath heating 2h, to be cooled to being transferred to after room temperature
It is placed in micro-wave oven microwave treatment 10min under 900W in beaker, is finally centrifuged, is filtered, washed, being dried to obtain biomass/oxidation
Iron complexes.
For the biomass carbon/ferric oxide composite material performance for detecting the method for the present invention preparation, carried out with half-cell method
Test, with the negative electrode material of above embodiments 1 and comparative example 1: PVDF(Kynoar)=90:10, comparative example 1: acetylene black:
Appropriate NMP(N- methyl-1-pyrrolidones is added in PVDF=80:10:10) be tuned into pulpous state, coating on copper foil, in 80 DEG C of pre-add
Negative electrode tab is made in 10 hours in heat 1 hour, then 120 DEG C of vacuum drying；It is to electrode, electrolyte 1mol with metal lithium sheet
LiPF6/ EC+DEC+DMC=1:1:1, microporous polypropylene membrane are diaphragm, are assembled into battery.Charging/discharging voltage is 0.05V-3.0V,
Battery performance is tested.
Claims (6)
1. a kind of biomass carbon/ferric oxide composite material, it is characterised in that:
Including biomass carbon substrate and the iron oxide being attached in substrate, the iron oxide is distributed in the porous knot of biomass carbon
In structure, wherein biomass carbon accounting 20%~50%.
2. biomass carbon/ferric oxide composite material according to claim 1, which is characterized in that in the composite material
The porous structure of biomass carbon, hole diameter are 7~10um.
3. biomass carbon/ferric oxide composite material according to claim 1, which is characterized in that in the composite material
Iron oxide is rodlike, 50~150nm of granular size, is in normal distribution in the two sides 70nm, is evenly distributed on the hole of biomass carbon
Among, form nanostructure.
4. a kind of biomass carbon/ferric oxide composite material preparation method prepared as described in claims 1 to 3 is any, special
Sign is, using forced hydro-thermal method that biomass carbon is compound with iron oxide, obtains the carbon-coated iron oxide forerunner of multiporous biological matter
Then presoma is improved iron oxide crystallinity by microwave treatment, it is multiple to obtain biomass carbon/iron oxide of the present invention by body
Condensation material.
5. the preparation method of biomass carbon/ferric oxide composite material according to claim 4, which is characterized in that including such as
Lower step:
(1) 0.1~1.5g biomass carbon is added to the NaH that 300~500ml concentration is 0.03~0.07 g/L2PO4Aqueous solution
In, the FeCl that 3.6~10.8ml concentration is 1~3mol/L is then added dropwise3Solution, oil bath heating stir 1~3h simultaneously；
(2) solution for taking out step (1) is allowed to be cooled to room temperature, is then placed in micro-wave oven the microwave treatment at 800~900W
Biomass carbon of the invention/iron oxide composite wood can be obtained finally by being centrifuged, being filtered, washed, drying in 10~20min
Material.
6. the preparation method of biomass carbon/ferric oxide composite material according to claim 5, which is characterized in that further include
The preparation method of biomass carbon, comprising the following steps:
(1) leaf collected, bark, chips and/or animal hair are cleaned with deionized water, with 0.5~1.5mol/L's
Potassium hydroxide solution impregnates 20~48h, is then placed in 70~90 DEG C of drying in drying box；
(2) sample of drying is collected in ceramic vessel, be placed in calcining furnace 800~950 DEG C of calcinings 2 under ar gas environment~
4h；
(3) it is then washed with the hydrochloric acid solution of 0.5~1.5mol/L and deionized water until the aobvious neutrality of filtrate PH, is placed on drying box
In dry 10~20h at 75~85 DEG C, be ground up, sieved after taking-up, biomass carbon can be obtained.
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Cited By (6)
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| CN109626370A (en) * | 2019-01-21 | 2019-04-16 | 青岛科技大学 | The preparation and its application of biomass-based porous carbon materials based on sycamore seed |
| CN112310371A (en) * | 2020-10-19 | 2021-02-02 | 华东理工大学 | Iron oxyhydroxide/biomass charcoal composite material and preparation method thereof |
| CN113421990A (en) * | 2021-05-28 | 2021-09-21 | 西安理工大学 | Iron-based biomass carbon intermediate layer of lithium-sulfur battery, preparation method and lithium-sulfur battery |
| CN114388737A (en) * | 2021-12-24 | 2022-04-22 | 西安理工大学 | Self-supporting electrode, preparation method thereof and lithium-sulfur battery |
| CN114709405A (en) * | 2022-04-27 | 2022-07-05 | 深圳市寒暑科技新能源有限公司 | Preparation method of biomass-based hard carbon composite material |
| CN114751393A (en) * | 2022-03-27 | 2022-07-15 | 上海市质量监督检验技术研究院 | Nitrogen-sulfur co-doped porous carbon/sulfur composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109626370A (en) * | 2019-01-21 | 2019-04-16 | 青岛科技大学 | The preparation and its application of biomass-based porous carbon materials based on sycamore seed |
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| CN113421990A (en) * | 2021-05-28 | 2021-09-21 | 西安理工大学 | Iron-based biomass carbon intermediate layer of lithium-sulfur battery, preparation method and lithium-sulfur battery |
| CN114388737A (en) * | 2021-12-24 | 2022-04-22 | 西安理工大学 | Self-supporting electrode, preparation method thereof and lithium-sulfur battery |
| CN114751393A (en) * | 2022-03-27 | 2022-07-15 | 上海市质量监督检验技术研究院 | Nitrogen-sulfur co-doped porous carbon/sulfur composite material and preparation method and application thereof |
| CN114709405A (en) * | 2022-04-27 | 2022-07-05 | 深圳市寒暑科技新能源有限公司 | Preparation method of biomass-based hard carbon composite material |
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